反应详情

温度

120 °C

Cs2CO3 (5 eq, 1.45 mmol, 480 mg) and 4A molecular sieves (400 mg) are stirred in a mixture of DMSO (5 ml) and ethanol (5 eq 0.8 ml). To this suspension is added [4-[3-(2-chloro-pyridin-4-yl)-imidazo[1,2-a]pyridin-6-ylamino]-cyclohexanol (Example 2.1) (1 eq, 100 mg, 0.29 mmol). The reaction is heated at 120° C. for 16 hours. The mixture is diluted with H2O (20 ml) and extracted with EtOAc. The combined organic portions are washed with brine, dried (MgSO4) and concentrated in vacuo to give a blue oil. The residue is purified by flash chromatography on silica eluting with 0-10% methanol in EtOAc The resulting residue is loaded onto a SCX-2 cartridge (resin loading 0.67 mmol/g) eluting with MeOH followed by 2M NH3 in MeOH. The methanolic ammonia fractions are concentrated in vacuo and dried under vacuum to afford the title compound; [M+H]+=353

1. extractionextracted with EtOAc
2. washThe combined organic portions are washed with brine
3. dry with materialdried (MgSO4)
4. concentrationconcentrated in vacuo
5. customto give a blue oil
6. customThe residue is purified by flash chromatography on silica eluting with 0-10% methanol in EtOAc The resulting residue
7. washeluting with MeOH
8. concentrationThe methanolic ammonia fractions are concentrated in vacuo
9. customdried under vacuum